耿丽婵 皮业华 杨亮改

摘要：地表水中硫化物的测定受水体本身浊度和色度的影响比较大，本文提出了利用凯式蒸馏使硫化物迅速逃逸后被氢氧化钠为吸收液吸收，再用亚甲基蓝分光光度法测定吸收液中的硫化物方法，并对该方法的具体操作过程进行了详述，对方法的检出限、精密度、准确度进行了评价确认。本文是对GB/T 16489-1996《水质 硫化物的测定 亚甲基蓝分光光度法》的优化与改进。新方法具有操作简便、成本低、蒸馏效率稳定的优势。与多联数显恒温电热套联合使用，易于实现大批次样品的快速检测，具有推广使用的价值。

关键词：水质硫化物  非氮吹系统  凯式加热蒸馏  亚甲基蓝分光光度法

Application Example of Non - Blowing System for Determination of Sulfide in Surface Water

GEN Lichan  PI Yehua  YANG  Lianggai

（First Geological Brigade， Hubei Provincial Bureau of Geology， Daye， Hubei  Province， 435100 China）

Abstract： The determination of sulfide in surface water is greatly affected by the turbidity and chromaticity. This paper presents a method of using Kay distillation to make the sulfide escape quickly and be absorbed by sodium hydroxide as absorption solution， and then using methylene blue spectrophotometry to determine the sulfide in absorption solution.The specific operation process of the method is described in detail， and the detection limit， precision and accuracy of the method are evaluated and confirmed.This paper is an optimization and improvement of GB/T 16489-1996 Methylene Blue Spectrophotometric Method for Determination of Sulphide in Water Quality.The method has many advantages such as simple operation， low cost and stable distillation efficiency. This method can be used with a multi-unit digital display thermostat electric jacket， the rapid detection of large batches of samples can be achieved， and the value of popularization can be provided.

Key Words： Sulfide in surface water; Non-nitrogen blowing system; Kjeldah heating separation method; Methylene blue colorimetric method

硫化物的大量存在会导致水生生物死亡，加快金属管路的腐蚀。人体吸入硫化氢后破坏人体细胞，吸入过量会导致人在短时间内死亡。因此，对水体中硫化物含量的监测是判断水质污染状况的重要指标。目前，文献报道的硫化物的测定方法很多，但被國家/行业认可的方法只有碘量法[1]、亚甲基蓝分光光度法[2]、离子色谱法[3]、气相分子吸收光谱法[4]和流动注射-亚甲基蓝分光光度法[5]等。碘量法的检出限较高，适用于分析硫化物浓度比较高的样品。国内外测定硫化物最常用的方法为亚甲基蓝分光光度法，因为其具有灵敏度高、测试精密度好、选择性好的优点[6]。离子色谱法和气相分子吸收光谱法需要的设备相比前两种更昂贵。第三方检测实验室在没有配备离子色谱仪或者气相分子吸收光谱仪的情况下，大多采用的是碘量法和分光光度法。……